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Hydrochloric Acid → HCID 20186762、化合物

HRID 1594372
ノート
印刷プレビュー

反応式

HRID 1594372 の反応式
[C:1]1([CH:7]([O:10][CH2:11][CH2:12][O:13][Si](C)(C)C)[C:8]#[N:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl>>[NH2:9][CH2:8][CH:7]([C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)[O:10][CH2:11][CH2:12][OH:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 313Hydrochloric AcidHCID 13099198α-[2-[(Trimethylsilyl)oxy]ethoxy]benzeneacetonitrile

生成物 1

HCID 20186762HCID 20186762、化合物収率 89.5%

実験手順

To a 100 ml three-necked flask, 1.0 g (4.01 mmol) of Compound 2 was added and the atmosphere was changed to nitrogen after degassing. The flask was dipped in an ice bath and 30 ml of 1M BH3 solution in THF was slowly added. The resulting mixture was stirred for 30 minutes while cooling the mixture in ice and then at room temperature for 4 hours. After completion of the reaction, the reaction vessel was dipped in an ice bath and aqueous 1N HCl solution was added, thereby making the mixture acidic. After evaporating the solvent under reduced pressure, 20 ml of water was added and aqueous NaOH solution was added to adjust the pH to 10. The mixture was extracted with ethyl acetate and the organic phase was washed with water, followed by drying over anhydrous sodium sulfate to obtain a colorless oily compound (650 mg, Yield: 89.5%).

後処理

  • customafter degassing
  • customThe flask was dipped in an ice bath
  • addition30 ml of 1M BH3 solution in THF was slowly added
  • temperaturewhile cooling the mixture in ice
  • waitat room temperature for 4 hours
  • customAfter completion of the reaction
  • customthe reaction vessel was dipped in an ice bath
  • customAfter evaporating the solvent under reduced pressure, 20 ml of water
  • additionwas added
  • additionaqueous NaOH solution was added
  • extractionThe mixture was extracted with ethyl acetate
  • washthe organic phase was washed with water
  • dry with materialby drying over anhydrous sodium sulfate
  • 出典と根拠

    ORDレコード
    ord-1d14cb96dd1f4ff38d0a7fe8bab838ec
    出典データセット
    uspto-grants-2007_11
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US07301018B2

    反応ノート

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